WO2006123049A2 - Elaboration par voie electrolytique d'elements nanocomposites conducteurs auto-supportes - Google Patents
Elaboration par voie electrolytique d'elements nanocomposites conducteurs auto-supportes Download PDFInfo
- Publication number
- WO2006123049A2 WO2006123049A2 PCT/FR2006/001099 FR2006001099W WO2006123049A2 WO 2006123049 A2 WO2006123049 A2 WO 2006123049A2 FR 2006001099 W FR2006001099 W FR 2006001099W WO 2006123049 A2 WO2006123049 A2 WO 2006123049A2
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- Prior art keywords
- substrate
- nanowires
- metal
- cathode
- composite element
- Prior art date
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- 238000000034 method Methods 0.000 title claims abstract description 61
- 238000004519 manufacturing process Methods 0.000 title description 3
- 239000002114 nanocomposite Substances 0.000 title description 2
- 239000000758 substrate Substances 0.000 claims abstract description 82
- 239000012528 membrane Substances 0.000 claims abstract description 69
- 239000002070 nanowire Substances 0.000 claims abstract description 62
- 239000002131 composite material Substances 0.000 claims abstract description 41
- 229910052751 metal Inorganic materials 0.000 claims abstract description 41
- 239000002184 metal Substances 0.000 claims abstract description 40
- 239000002243 precursor Substances 0.000 claims abstract description 29
- 239000003792 electrolyte Substances 0.000 claims abstract description 23
- 239000007769 metal material Substances 0.000 claims abstract description 17
- 239000004020 conductor Substances 0.000 claims abstract description 10
- 150000003839 salts Chemical class 0.000 claims abstract description 8
- 125000006850 spacer group Chemical group 0.000 claims abstract description 7
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- 229910052802 copper Inorganic materials 0.000 claims description 35
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- 238000005868 electrolysis reaction Methods 0.000 claims description 12
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 8
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- 229910006404 SnO 2 Inorganic materials 0.000 claims description 4
- 229910052797 bismuth Inorganic materials 0.000 claims description 4
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- 229910018100 Ni-Sn Inorganic materials 0.000 claims description 3
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- 150000004820 halides Chemical class 0.000 claims description 2
- 150000004678 hydrides Chemical class 0.000 claims description 2
- 150000002739 metals Chemical class 0.000 claims description 2
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 2
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- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical class [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 2
- 239000005518 polymer electrolyte Substances 0.000 claims description 2
- IIACRCGMVDHOTQ-UHFFFAOYSA-N sulfamic acid Chemical class NS(O)(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-N 0.000 claims description 2
- 150000003467 sulfuric acid derivatives Chemical class 0.000 claims description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 claims description 2
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical class FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 claims description 2
- 150000003568 thioethers Chemical class 0.000 claims description 2
- QHGNHLZPVBIIPX-UHFFFAOYSA-N tin(II) oxide Inorganic materials [Sn]=O QHGNHLZPVBIIPX-UHFFFAOYSA-N 0.000 claims description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims 1
- 229910016345 CuSb Inorganic materials 0.000 claims 1
- 229910017052 cobalt Inorganic materials 0.000 claims 1
- 239000010941 cobalt Substances 0.000 claims 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims 1
- 239000010949 copper Substances 0.000 description 38
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 28
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- 239000012691 Cu precursor Substances 0.000 description 2
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- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
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- 239000010936 titanium Substances 0.000 description 2
- 229910001152 Bi alloy Inorganic materials 0.000 description 1
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 1
- 239000012692 Fe precursor Substances 0.000 description 1
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 1
- 229910052493 LiFePO4 Inorganic materials 0.000 description 1
- 229910015645 LiMn Inorganic materials 0.000 description 1
- 229910013290 LiNiO 2 Inorganic materials 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000002313 adhesive film Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000003490 calendering Methods 0.000 description 1
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- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
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- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/02—Electroplating of selected surface areas
- C25D5/022—Electroplating of selected surface areas using masking means
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D1/00—Electroforming
- C25D1/006—Nanostructures, e.g. using aluminium anodic oxidation templates [AAO]
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D1/00—Electroforming
- C25D1/04—Wires; Strips; Foils
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/134—Electrodes based on metals, Si or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/661—Metal or alloys, e.g. alloy coatings
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/70—Carriers or collectors characterised by shape or form
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/70—Carriers or collectors characterised by shape or form
- H01M4/75—Wires, rods or strips
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/045—Anodisation of aluminium or alloys based thereon for forming AAO templates
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
- H01L2924/0001—Technical content checked by a classifier
- H01L2924/0002—Not covered by any one of groups H01L24/00, H01L24/00 and H01L2224/00
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/12—All metal or with adjacent metals
- Y10T428/1241—Nonplanar uniform thickness or nonlinear uniform diameter [e.g., L-shape]
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/12—All metal or with adjacent metals
- Y10T428/12431—Foil or filament smaller than 6 mils
- Y10T428/12438—Composite
Definitions
- the invention relates to a method for depositing a nanostructured metal coating on an electronically conductive substrate, and the coated substrates obtained.
- the properties of the electrodes, and in particular the current collectors that the electrodes comprise are an important element for the overall performance of the batteries.
- a material to be used as a collector it is desirable that it has a high electronic conductivity, good electrochemical stability, and a large contact area with the active material.
- Nanomaterials have a large surface area to volume ratio, which leads to an increase in reaction rates by decreasing diffuse limitations, and the use of nanomaterials for the elaboration of current collectors is under development.
- nanostructured electrical conducting materials in the form of solid or hollow fibers using a porous membrane, electrochemically or chemically.
- a chemical method is described in particular by B. Bercu, et al. [Nuclear Instruments and Methods in Physics Research B 225 (2004) 497-502].
- the method involves activating a polycarbonate membrane and then contacting it with a copper precursor solution. After sufficient contact time for copper to be deposited on the pore walls of the membrane and further form a layer on the surface of the membrane, the membrane is removed by dissolution, and a self-supported member is obtained. consisting of a copper layer carrying on its surface nano-elements in the form of hollow copper nanotubes.
- the copper layer forming a substrate obtained by electrochemical and / or chemical deposition for the nano-elements is necessarily porous, and the length of the nano-elements in the self-supported element final is imposed by the thickness of the membrane, since the formation of the copper film on the surface of the membrane begins only when the surface of the pores of the membrane is completely covered with copper.
- the fact that the copper nanoelements carried by the copper substrate are hollow is unfavorable to the mechanical strength of the self-supported element, as well as to its use as current collector, the amount of current conveyed through the hollow elements being less than with full nanoelements.
- D. Dobrev, et al. [Nuclear Instruments and Methods in Physics Research B 149 (1999) 207-212] discloses a method for electrochemically forming nanoscale metal needles using a membrane porous.
- the method consists of PVD coating an Au conductive film on one side of a polycarbonate membrane, electrochemically depositing a layer of copper on the Au conductive film, and then depositing copper in the pores of the membrane by the face of the membrane remained free, and finally dissolve the membrane with a suitable solvent.
- the self-supported element obtained is constituted by a copper substrate carrying nanoscale copper needles, an Au film being interposed between the copper substrate and the nanoscale needles.
- the object of the present invention is to provide a method which makes it possible to obtain a self-supported composite element consisting of an electronically conductive substrate coated with nanostructured metal elements, which does not have the drawbacks of the processes of the prior art.
- the subject of the present invention is a method of producing a self-supported element, the self-supported composite element obtained, as well as various applications.
- the method according to the present invention for obtaining a self-supported composite element consisting of a non-porous conductive substrate coated with nanowires of metallic material, consists of electrolytic deposition on a substrate through a porous membrane, then to dissolve the porous membrane.
- an electrochemical cell connected to a source of voltage and / or controlled current, and comprising: a cathode formed by the non-porous electronic conductive substrate to be coated, and connected to the negative terminal of the voltage and / or current source, one or more anodes, each connected to the positive terminal of the voltage and / or current source, an electrolyte consisting of a solution of a precursor compound of each constituent of the metallic material, said solution optionally containing an ionically conductive salt, a planar porous membrane placed on the face or faces of the cathode, a spacer element between each membrane and the anode adjacent thereto, the different parts constituting the cell being kept in contact.
- the different parts constituting the cell can be kept in contact by pressure.
- the contact can result from the gravity.
- the electrolysis can be carried out at constant, pulsed, alternating or oscillating current, or under constant potential, impulse, alternating or oscillating, or under constant power, impulse, alternating or oscillating.
- the precursor of a component of the metallic material MM constituting the nanowires may be a precursor of a metal M, said metal M being selected from Cu, Sn, Co, Fe, Pb, Ni, Cr, Au, Pd, Pt, Ag , Bi, Sb, Al or Li.
- M is Al or Li
- the precursor is used in solution in an organic solvent.
- M is Cu, Sn, Co, Fe, Pb, Ni, Cr, Au, Pd, Pt, Sb, Ag or Bi
- the precursor may be used in aqueous solution or in solution in an organic solvent.
- the precursor is preferably chosen from sulphates, sulphamates, borates, halides (more particularly chlorides and fluorides), complexes based on cyanides or amines, and hydrides.
- the organic solvent is preferably chosen from alkyl or dialkyl carbonates, such as, for example, propyl carbonate (PC), ethyl carbon (EC) and diethyl carbonate (DEC).
- a complexing agent of the precursor of the metal M to be deposited is introduced into the electrolyte, in order to reduce the kinetics of the reduction of the metal M, which makes it possible to obtain a uniform and covering deposit.
- the ionic conductive salt of the electrolyte is chosen from electrochemically stable conductive salts under the conditions of electrolysis. It can be a salt of the metal to be deposited.
- the addition of an ionic conductive salt is not essential. However, for low precursor concentrations, the conductivity of the electrolyte is low, or even insufficient, and in this case it is useful to add a conductive salt to the electrolyte.
- the cathode is made of a non-porous electronic conductive material selected from materials that are chemically stable to electrolysis. Mention may be made, for example, of metal materials MM 'consisting of a metal M' chosen from Li, Zn, Cu, Sn, Co, Fe, Pb, Ni, Ti, Cr, Al, noble metals such as for example Au, Ag, Pd and Pt, or a metal alloy of several elements M '. It is particularly advantageous to use as a cathode a sheet of material obtained by rolling, drawing, calendering or stamping.
- the metal sheet may for example be in the form of a flat sheet, an accordion folded sheet. At least one of the two faces of the sheet constituting the cathode is facing an anode.
- the electrochemical cell contains a cathode whose only one of the faces is opposite an anode.
- the deposition of nanowires then takes place, during the electrolysis, on the face of the cathode opposite the anode.
- the electrochemical cell contains two anodes in the form of thin sheets, located on either side of a metal sheet constituting the cathode.
- the sheets constituting the anodes are parallel to the sheet forming the cathode.
- the deposit nanowires are then carried out simultaneously on both sides of the cathode.
- a cathode constituted by a metal M 'identical to the metal M of the precursor of the nanowires is used.
- the particular case of a copper cathode and a copper precursor is particularly interesting.
- the porous membrane may be constituted for example by a sheet of alumina, in which the pores are substantially in the form of nanometric cylinders perpendicular to the plane of the membrane, by a polycarbonate sheet (PC) or by a sheet of terephthalate (PET) .
- Organic material sheets generally include less regular and less ordered pores than alumina sheets.
- the length of the nanowires formed in the pores of the membrane depends in particular on the duration of the electrolysis and the content of the precursor electrolyte of the metal to be deposited.
- the membrane will be chosen so that its thickness is greater than or equal to the desired length for the nanoparticles.
- Alumina membranes in which the pores are substantially cylindrical, perpendicular to the surface of the member and uniformly distributed are obtained by anodic oxidation of aluminum. They are marketed in particular under the name Anodisc by the company Whatman.
- the PC or PET membranes can be obtained by pre-sensitizing a PC or PET sheet, followed by perforation using a laser.
- PET membranes are marketed in particular by Whatman under the names Cyclopre and Nucleopore.
- PC membranes are sold in particular by the said company under the name Whatman Polycarbonate.
- the polycarbonate membranes generally have sufficient mechanical strength so that the spacer element can be a simple element for creating a space between the membrane and the anode, said space containing the electrolyte.
- the alumina membranes generally have a low mechanical strength, and it is preferable to associate them with a spacer element of the separator type, constituted by a sheet of an ionic conductive material and electronic insulator.
- a separator there may be mentioned a porous sheet of cellulosic or polymeric material.
- the separator has the effect not only of improving the mechanical strength of the membrane which is adjacent to it, but also of increasing the homogeneity of the deposition of nanowires, because of the penetration of the electrolyte by capillarity into the membrane, this which has the effect of preventing the drying of the membrane.
- the use of a membrane makes it possible to have smaller inter-electrode distances than with a spacer.
- the use of a non-continuous porous membrane makes it possible to obtain a self-supported element consisting of a non-porous electronic conductive substrate bearing a coating of nanotructured elements, in which the coating of nanowires is not continuous.
- a porous membrane is brought into contact with said substrate in the surface of which recesses are formed, said recesses having the shape and the area of the areas of the surface of the substrate which are intended not to be coated. by the nanowires and which are masked before the electrolysis, so as not to suffer the effects of the electrolytic process.
- the solid parts of the membrane are the image of the areas of the substrate that will be coated with nanoparticles.
- the anode may be soluble anode type, consisting of a metal identical to the metal M of the nanowire precursor, which makes it possible to maintain a constant concentration of metal ions M in the solution and to limit the voltage across the cell.
- the anode may also be constituted by an indestructible metallic conductor in the solution on which will then be the oxidation of the solvent.
- the anode may also be of the soluble anode type consisting of a material other than the metal to be deposited, but in this case the conditions of the electrolysis must be adjusted so as to avoid the deposition on the cathode of an alloy. metal M and the material constituting the anode.
- This product is a self-supported composite element constituted by a non-porous substrate of electronically conductive material which carries, on at least one of its faces, a coating constituted by nanowires of a metallic material, said nanowires being substantially oriented in a plane perpendicular to the substrate.
- the thickness and shape of the substrate correspond to those of the cathode used for the preparation of the composite element.
- the thickness of the substrate is preferably less than 1 mm, for example 5 ⁇ m and 500 ⁇ m.
- the substrate may be in the form of a flat sheet, an accordion folded sheet, or a folded sheet to form the side walls of a cylinder having, for example, a triangular section or a quadrilateral section.
- a self-supported composite element according to the present invention differs from similar elements of the prior art in which the substrate is obtained by electrochemical deposition or electroless over a porous membrane, not only by the absence of porosity, but also by grain orientation and roughness.
- the material forming the substrate is deposited in the form of islands whose orientation is substantially perpendicular to the plane of the substrate.
- the roughness is oriented in the direction perpendicular to the plane of the substrate.
- the general orientation of the roughness and grains is parallel to the plane of the substrate. These substrates therefore have a particular texture oriented in the rolling plane which is not the case in other electroless or electrochemical processes.
- the conductive material forming the substrate of the composite element is as defined above for the cathode of the electrochemical cell used during the implementation of the process for preparing the composite element.
- the metallic material forming the nanowires is constituted by a metal M chosen from Cu, Sn, Co, Fe, Pb, Ni, Cr, Au, Pd, Pt, Ag, Bi, Sb, Al or Li, or by an alloy of several metals M.
- the length of the nanowires depends on the one hand on the length of the pores of the membrane and on the other hand on the duration of the electrolysis. It is generally between a few hundred nanometers and a few tens of micrometers, for example from 500 nm to 100 ⁇ m.
- a membrane constituted by an alumina sheet in which the pores are substantially cylindrical and oriented perpendicularly to the surface of the plate forming the membrane, makes it possible to obtain a substrate coated with substantially cylindrical elements oriented perpendicularly. on the surface of the substrate.
- PC or PET membrane gives a coating consisting of cylindrical elements which are less regular and less oriented with respect to the surface of the substrate, due to a less regular pore distribution in this type of membrane.
- the substrate may have a coating of nanowires on only one of its faces, or on both sides.
- a face of the substrate may carry a coating of nanowires on its entire surface, or in certain areas only.
- a composite element according to the present invention can be used either as a current collector or as an electrode, depending on the nature of the materials which constitute on the one hand the substrate and on the other hand the coating formed by the nanowires.
- the substrate is preferably formed by a thin film of conductive material having a thickness of a few tens to a few hundred micrometers.
- the present invention therefore has for another object, a current collector and an electrode comprising said composite element.
- a self-supporting composite member according to the present invention wherein the metal material MM constituting the nanowires has electrode active material properties, can be used directly as an electrode, without adding additional active material.
- a composite element there may be mentioned a composite element in which the substrate is constituted by a material MM 'chosen from Cu, Al, Li, Pb, Zn, Ni, Ti, Au, Ag Pt or Pd, and the material metallic MM constituting the nanowires is selected from Sn, Li, and the alloys Ni 3 Sn, Mg 2 Sn and Cu 2 Sb.
- a self-supported composite member according to the present invention wherein the metal material MM constituting the nanowires does not have electrode active material properties, can be used as a current collector of an electrode.
- the substrate and the coating of nanowires are preferably constituted by the same metal, chosen from Cu, Al, Li, Pb, Zn, Ni, Au, Ag Pt or Pd.
- the current collector can be converted into an electrode by subjecting the nanowire coating to oxidation.
- a self-wearing element is thus obtained constituted by the substrate of initial material MM 'and by a coating of oxide nanowires with properties of active material.
- an electrode comprising a substrate of a material MM 'carrying a coating of tin oxide nanowires SnO or SnO 2 , iron oxide FeO, Fe 2 O 3 or Fe 3 O 4 , nickel oxide or cobalt oxide, obtained from a composite element according to the invention which comprises a substrate of the material MM 'and a coating of nanowires respectively of Sn, Fe, Ni or Co.
- an electrode is made from a current collector according to the invention by depositing electrode active material on the nanowire coating.
- the deposition of the electrode active material on the current collector can advantageously be carried out electrolytically in an electrochemical cell in which the composite element functions as a cathode, and the electrolyte is constituted by a precursor of the active material, in conditions that are within the reach of the skilled person.
- an electrode comprising a collector consisting of a copper substrate coated with copper nanowires, on which an Sn film has been applied by electrolysis.
- the deposition of active material may also be carried out by impregnation or by coating, when the size of the particles of active material is less than the distance between the nanowires.
- the active ingredient may also be deposited by sol-gel, if the size of the particles to be deposited is less than the distance between the nanowires.
- the active material can also be deposited physically, by growth of thin layers, for example by sputtering or laser ablation techniques.
- Current collectors and electrodes according to the invention can be used in various electrochemical devices such as rechargeable lithium-ion batteries, rechargeable lithium-polymer batteries, non-rechargeable generators, supercapacitors, and electrochromic devices.
- a lithium ion battery comprises a negative electrode and a positive electrode separated by a liquid or gelled electrolyte comprising a lithium salt.
- Each of the electrodes consists of a material capable of reversibly inserting lithium ions.
- the positive electrode of a lithium-ion battery may consist of a current collector comprising an Al substrate bearing a coating of Al nanowires, and an active material consisting of a lithiated oxide such as LiCoO 2 , LiNiO 2 or LiMn 2 O ,! , or a phosphate such as LiFePO4.
- active substances can be deposited on the collector AI / AI advantageously by impregnation or by coating.
- the negative electrode of a lithium-ion battery may be constituted by Cu collector, and an active material selected from Sn, SnO 2 , Bi, a Ni-Sn alloy, an Sb-based alloy, an Fe oxide, Co or Ni.
- An electrode comprising, as Sn active material, a Ni-Sn or Bi alloy may advantageously be obtained by implementing the method of the invention with a copper substrate and an electrolyte respectively containing a Sn precursor, a mixture of a precursor of Sn and a precursor of Ni, or a precursor of Bi.
- An electrode comprising as active material an Sn, Fe, Co or Ni oxide can advantageously be obtained by implementing the method of the invention with a copper substrate and an electrolyte respectively containing a Sn, Fe or Fe precursor. , Co or Ni or to obtain a composite element comprising a Cu substrate and metal nanowires corresponding to the precursor chosen, then subjecting the composite element to oxidation in the appropriate conditions
- a lithium polymer battery comprises a negative electrode and a positive electrode separated by a solid polymer electrolyte comprising a lithium salt.
- the anode consists of a metallic lithium film or a lithium alloy.
- the cathode may advantageously be an electrode according to the invention comprising a current collector consisting of an Al substrate bearing Al nanowires and a positive electrode active material chosen from the lithiated oxides mentioned for the positive electrode of the cathode.
- a positive electrode active material chosen from the lithiated oxides mentioned for the positive electrode of the cathode.
- lithium-ion battery and among non-lithiated oxides, such as for example V 2 O 5 , said active material being advantageously deposited by impregnation or by coating.
- a self-supported composite element according to the present invention may advantageously be used for producing an electrode in a non-rechargeable battery in which the electrolyte comprises a lithium salt in solution in a liquid solvent.
- the anode consists of a metallic lithium film or a lithium alloy.
- the cathode may advantageously be an electrode according to the invention comprising a current collector consisting of an Al substrate bearing Al nanowires and a positive electrode active material chosen from oxides, such as, for example, V 2 O 5 , WO 3 or MnO 2 , sulfides such as FeS 2 or CF x carbon fluorides.
- a supercapacitor comprises two electrodes separated by an electrolyte.
- One of the electrodes is preferably made of a material with a high specific surface area.
- Such an electrode may advantageously be an electrode according to the invention comprising a current collector consisting of an Al substrate bearing Al nanowires, or a Cu substrate carrying Cu nanowires, and an active material consisting for example of carbon, or a polymer.
- a composite element according to the present invention may furthermore be used in power electronics, and more generally in microelectronics, as part of the connection of the active components with their environment or as a heat sink element, the two functions being combinable.
- the method of the invention is implemented using as cathode the surface of a semiconductor element with at least one * of the faces is at least partially covered by a metallization, and the membrane is placed on all or part of the metallization of the semiconductor element.
- a mask is applied to the free surface of the membrane so as to delimit zones of the semiconductor element which will be covered with nanowires.
- This embodiment allows the use of the method on the entire surface of a semiconductor wafer at the end of the process in a clean room (front end process).
- the use of a membrane carrying a mask makes it possible to create the pads of connection (commonly referred to in the technical field literature as "studs” or “bumps") on a semiconductor element.
- the semiconductor element will then be attached to another semiconductor element or element of the environment by means well known to those skilled in the art, such as glues, solders or solders, or adhesive films (commonly referred to in the technical literature as “solders” or “tapes”).
- the attachment may further be effected by direct methods such as a thermocompression method or a thermosonic process.
- the choice of the method of attachment will depend, among other things, on the type of metal alloy used for the manufacture of the pads and the receiving support (semiconductor element or element of the environment).
- PCB Printed Circuit Board or Printed Circuit Board
- PCB Printed Circuit Board or Printed Circuit Board
- An inorganic carrier is generally referred to as a "substrate”
- an organic carrier such as epoxy resin / fiberglass (type FR4)] is referred to as "PCB”.
- the copper foils forming respectively the cathode and the anode have a thickness of 500 microns.
- the alumina membrane is a membrane marketed under the name Anodisc by the company Whatman. It has a thickness of 50 ⁇ m and the diameter of the substantially cylindrical pores is 200 nm.
- the electrolyte is an aqueous solution of CUSO 4 (100 g / L), (NH 4 ) 2 SO 4 (20 g / L) and diethylenetetetamine DETA (80 g / L).
- the electrolysis was carried out under current pulses by repeating the sequence "deposition at 1 mA / cm 2 for 250 ms, deposition at 20 mA / cm 2 for 50 ms" for 30 minutes.
- a diagram of the device used is shown in FIG. 1, in which (1) represents the electrolyte, (2) represents the cathode, (3) represents the membrane, (4) represents the separator, (5) represents the anode , and (6) represents the potentiostat.
- the cell was disassembled. The assembly formed by the cathode and the alumina membrane was immersed in a 1M sodium hydroxide solution at 80 ° C. for 30 seconds. After dissolution of the membrane, the cathode was rinsed for 10 seconds in an aqueous solution of H 2 SO 4 (1 M) and CuSO 4 (1 M).
- Figures 2 to 4 show a view of the product facing the ends of the nanocylinders, with different magnifications (x 1000, x 10000, x 100000), and Figure 5 shows a sectional view, with a magnification of 30000.
- Example 1 The procedure of Example 1 was repeated using: • a Cu sheet having a thickness of 500 ⁇ m forming the cathode, • Anodisc alumina membrane
- the electrolyte is an aqueous solution containing SnSO 4 (97 g / L), HSO 4 (30 g / L), tartaric acid (30 g / L), polyethylene glycol PEG 3500 (0.35 g / L) ), gelatin (1 g / L) and Na 2 SO 4 (30 g / L).
- the electrolyte is an aqueous solution containing SnSO 4 (97 g / L), HSO 4 (30 g / L), tartaric acid (30 g / L), polyethylene glycol PEG 3500 (0.35 g / L) ), gelatin (1 g / L) and Na 2 SO 4 (30 g / L).
- Figure 6 shows a SEM-FEG photograph of the product obtained.
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Abstract
Description
Claims
Priority Applications (3)
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US11/920,624 US9115438B2 (en) | 2005-05-18 | 2006-05-16 | Method for the electrolytic production of self-supporting conductive nanocomposite elements |
EP06764636A EP1885916A2 (fr) | 2005-05-18 | 2006-05-16 | Elaboration par voie electrolytique d'elements nanocomposites conducteurs auto-supportes |
JP2008511749A JP5148481B2 (ja) | 2005-05-18 | 2006-05-16 | 自立伝導性ナノ複合エレメントの電解製造法 |
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FR0504960A FR2885913B1 (fr) | 2005-05-18 | 2005-05-18 | Element composite comprenant un substrat conducteur et un revetement metallique nanostructure. |
FR0504960 | 2005-05-18 |
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WO2006123049A2 true WO2006123049A2 (fr) | 2006-11-23 |
WO2006123049A3 WO2006123049A3 (fr) | 2007-12-06 |
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PCT/FR2006/001099 WO2006123049A2 (fr) | 2005-05-18 | 2006-05-16 | Elaboration par voie electrolytique d'elements nanocomposites conducteurs auto-supportes |
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US (1) | US9115438B2 (fr) |
EP (1) | EP1885916A2 (fr) |
JP (1) | JP5148481B2 (fr) |
FR (1) | FR2885913B1 (fr) |
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Also Published As
Publication number | Publication date |
---|---|
JP5148481B2 (ja) | 2013-02-20 |
WO2006123049A3 (fr) | 2007-12-06 |
US9115438B2 (en) | 2015-08-25 |
FR2885913A1 (fr) | 2006-11-24 |
FR2885913B1 (fr) | 2007-08-10 |
JP2008545881A (ja) | 2008-12-18 |
US20090316335A1 (en) | 2009-12-24 |
EP1885916A2 (fr) | 2008-02-13 |
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